13C4-Secobarbital as the Internal Standard for the Quantitative Determination of Secobarbital—A Critical Evaluation

    Volume 45, Issue 3 (May 2000)

    ISSN: 0022-1198

    CODEN: JFSOAD

    Page Count: 6


    Lin, D-L
    Scientific Staff, Scientific and Technical Research Center, Ministry of Justice Investigation Bureau, Taipei, Taiwan,

    Low, I-A
    Associate Professor and Professor, Central Police University, Taoyuan, Taiwan,

    Liu, RH
    Professor and Director, Graduate Program in Forensic Science, University of Alabama at Birmingham, Birmingham, AL

    Chang, W-T
    Associate Professor and Professor, Central Police University, Taoyuan, Taiwan,

    (Received 6 July 1999; accepted 24 August 1999)

    Abstract

    In this study, 13C4-secobarbital was used as an exemplar compound to illustrate the mechanism based on which the effectiveness of a proposed internal standard (IS) could be evaluated. A deuterated analog, 2H5-secobarbital, was also studied in parallel for comparison purposes. Well-established solid-phase extraction and methylation procedures were used prior to the GC/MS measurement step. The contribution of the intensity of an ion designated for the analyte (secobarbital) by the proposed IS, and similarly, the contribution of the intensity of an ion designated for the IS by the analyte—a phenomenon termed “cross-contribution”—were evaluated based on a “direct measurement” procedure in which equimolar amounts of the analyte and the IS were used to generate intensity data. These intensity data were then used as the basis for the calculation of “cross-contribution” (in percentages) of ions designated for the analyte and the IS. Cross-contribution data were compared with the linearity data resulting from two series of standards containing 25 to 9600 ng/mL secobarbital using two sets of quantitation ion pairs—m/z 196/200 and 195/199 with 13C4-secobarbital as the IS and m/z 196/201 and 195/200 with 2H5-secobarbital as the IS. 13C4-secobarbital was found to be much less problematic and thus can serve as a very effective IS. Cross-contribution data alone cannot fully explain the observed differences resulting from the use of these two ISs; further systematic study is needed to provide better understanding of the underlying interference mechanism.


    Paper ID: JFS14743J

    DOI: 10.1520/JFS14743J

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    Title 13C4-Secobarbital as the Internal Standard for the Quantitative Determination of Secobarbital—A Critical Evaluation
    Symposium , 0000-00-00
    Committee E30